SEPARATION PROCESSES IN THE FOOD AND BIOTECHNOLOGY INDUSTRIES Principles and Applications Edited by A. S. GRANDISON and M. J. LEWIS Department of Food Science and Technology University of Reading, UK WOODHEADP UBLISHING LIMITED Cambridge England Published by Woodhead Publishing Limited, Abington Hall, Abington, Cambridge CB 1 6AH, England First published 1996 0 1996, Woodhead Publishing Ltd Conditions of sale All rights reserved, No part of this publication may be reproduced or transmitted in any form or by any means, electronic or mechanical, including photocopy, recording or any information storage and retrieval system, without permission in writing from the publisher. While a great deal of care has been taken to provide accurate and current information, neither the author, nor the publisher, nor anyone else associated with this publication shall be liable for any loss, damage or liability directly or indirectly caused or alleged to be caused by this book. British Library Cataloguing in Publication Data A catalogue record for this book is available from the British Library ISBN I 85573 287 4 Typeset by Heather FitzGibbon, Christchurch, Dorset Printed by Galliard (Printers) Ltd, Great Yarmouth, England Preface This book concentrates on the more recent methods and techniques for separating food components and products of the biotechnology industry. Each chapter deals with a specific type or area of application and includes information on the basic principles, industrial equipment available, commercial applications and an overview of current research and development. The introductory chapter gives a brief overview of food composition and properties, and some of the heat and mass transfer considerations in batch and continuous processes. Separations from solids, liquids and gases are briefly discussed. A summary is provided of the more conventional separation techniques such as screening, filtration and centrifugation, and techniques for removing water, such as evaporation, freeze- concentration and dehydration. However, the main emphasis is on separation processes, which have received less attention in textbooks on food-engineering and food-processing operations. It is hoped that this book will complement and supplement many of these excellent texts. Chapter 2 deals with the use of supercritical fluids for extraction processes, with special reference to carbon dioxide. Chapter 3 deals with pressure- activated membrane techniques, and covers the general principles, reviews the applications of reverse osmosis, and serves as an introduction to Chapters 4 and 5, which deal specifically with the principles and applications of ultrafiltration and microfiltration respectively. The separation and recovery of charged particles by ion exchange and electrodialysis is covered in Chapter 6. Chapter 7 discusses innovative separation processes, and reviews some of the methods being actively investigated, some of which are now coming into industrial practice. Much of the emphasis in these chapters is on the separation and recovery of proteins and biologically active ingredients. Chapter 8 is specifically on the methods available for fractionating fat, and covers the upsurge in interest and recent developments in this area. The book concludes with a chapter on solids separation processes, with special reference to particulates. The physical properties which influence the separation are reviewed, together with sieving, screening and air classification. Wet processing methods for extraction are discussed, together with some miscellaneous applications such as dehulling, peeling and cleaning. xii Preface Much of the emphasis is on extraction of macromolecules, increasing the added value of foods and recovering valuable components from by-products and fermentation media. Many of the methods discussed are now in commercial practice, whilst others are being vigorously researched. A. S. Grandison and M. J. Lewis Contents ........................................................... Preface xi - .................................. 1 Separation processes an overview 1 A . S . Grandison and M . J . Lewis 1.1 Foods - the raw material ... ............................... 1 1.2 Separation techniques ... ............................... 5 1.2.1 Introduction ...... ............................... 5 1.2.2 Separations from solids ....................................... 7 Solid-solid separations ................................. 8 Separation from the solid matrix ............................ 9 1.2.3 Separations from liquids ..................................... 10 Liquid-solid separations ................................... 10 Immiscible liquids ........................................ 11 General liquid separation processes ........................... 11 1.2.4 Separations from gases and vapours ............................ 13 1.3 Water treatment ................................................. 15 1.4 References ..................................................... 15 .... 2 Supercritical fluid extraction and its application in the food industry 17 D . Steytler 2.1 Introduction ................. ............................... 17 2.2 The supercritical fluid state ..... ............................... 18 2.2.1 Physical properties of NCF CO, ............................... 20 Density ................................................ 20 Viscosity ............................................... 21 Diffusion ............................................... 22 Volatility (vapour pressure) ................................. 23 Chemical properties ...................................... 23 Biochemical properties ............................... 24 vi Contents 2.3 Properties of NCF solutions ....................................... 24 2.3.1 Solubilities in NCFs ........................................ 24 General principles ........................................ 25 Effect of molecular structure .............................. 25 Effect of temperature and pressure ......................... 28 2.3.2 Theoretical models (equations of state (EOS)) ..................... 28 Entrainers ............................................... 34 2.3.3 Diffusion coefficients ........................................ 35 2.4 Factors determining the efficiency of NCF extraction ................... 36 2.4.1 Extraction stage ............................................ 37 Mechanism of extraction ................................... 37 The ‘free diffusion’ model ................................ 38 The ‘shrinking core’ model ............................... 38 Solubility ............. ............................... 40 Diffusion coefficient ...................................... 40 Adsorption .............................................. 40 The role of water ......................................... 41 2.4.2 Separation stage ............................................ 42 2.5 Equipment and experimental techniques used in NCF extraction and fractionation ................................................... 44 2.5.1 Extraction ............... ........................ Pilot plants with recirculati ............................... 44 Small pilot plant with total loss of COZ ... 2.5.2 Fractionation .............................................. 46 Cascades of separation vessels .................... Zosel’s ‘hot finger’ fractionation column ................... 2.6 Applications .............................................. 2.6.1 Decaffeination of coffee and tea ............................... 49 2.6.2 Seed oil extraction .......................................... 51 2.6.3 Purification of lecithin ....................................... 52 2.6.4 Lowering cholesterol levels in foods ............................ 53 2.6.5 Fractionation of high-value oils and fats ......................... 53 Butterfat ................................................ 53 Fish oils ................. ............................ 54 2.6.6 Extraction of flavours and fragrances ........................... 54 2.7 References ..................................................... 57 ............................ 3 Pressure-activated membrane processes 65 M . J . Lewis 3.1 Introduction .................................................... 65 3.2 Terminology .................................................... 66 3.3 Concentration factor and rejection .................................. 69 3.4 Membrane characteristics ......................................... 70 3.5 Permeate rate ................................................... 71 3.6 Transport phenomena and concentration polarisation ................... 72 Contents vii 3.7 Membrane equipment ............................................ 75 3.7.1 Membrane configuration ..................................... 76 3.8 Safety and hygiene considerations .................................. 82 3.9 Reverse osmosis applications .................................... 86 3.9.1 Introduction ............................................... 86 3.9.2 Water treatment ............................................ 87 3.9.3 Milk processing ............................................ 88 3.9.4 Fruit and vegetable juices .................................... 90 3.9.5 Other applications ..... ........................... 91 3.10 References ................ ..................... .................................................. 4 Ultrafiltration 97 M . J . Lewis 4.1 Introduction .................................................... 97 4.2 Processing characteristics ......................................... 98 4.2.1 Rejection or retention factors ................................. 98 4.2.2 Yield ................ ................................. 101 4.2.3 Average rejection ...... ................................. 103 4.2.4 Practical rejection data ...................................... 104 4.3 Performance of ultrafiltration systems ............................... 105 Permeateflux ............................................ 105 4.3.1 Transport phenomena and concentration polarisation .......... . 106 4.3.2 Fouling ................ ........................... 111 4.3.3 Factors affecting flux ... ............................... 114 Energy input ....... ........................... 114 4.4 Diafiltration .................................................... 116 Introduction ............................................. 116 4.4.1 Washing out at constant volume ............................... 116 Washing-in ............................................. 118 4.4.2 Diafiltration applications ... ............................ 119 4.4.3 Protein fractionation ............................. 4.5 Ultrafiltration applications ... ... ............... 4.5.1 Dairy applications . . ........................... 4.5.2 Oilseed and vegetable proteins ............................ 125 4.5.3 Animal products ........................................... 127 4.5.4 Biotechnology applications ................................... 128 Membrane-based bioreactors ............................... 128 Enzyme reactors ......................................... 128 Membrane fermenters ..................................... 131 Recovery of components and downstream processing ............ 132 4.5.5 Medical applications: serum fractionation ......................... 133 4.6 References ..................................................... 134 viii Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Microfiltration , , , 141 A. S. Grandison and T. J. A. Finnigan 5.1 Introduction .................................................... 141 5.2 Theory, materials and equipment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 141 , , , , 5.2.1 Membrane configurations and characteristics . . . . . . . . . . . . . . . . 142 , , , , , 5.2.2 Performance of microfiltration systems and membrane fouling . . . . . . . 146 5.3 Applications in the food and biotechnology industries . . . . , . . . , . . . . . . . . . . 148 5.3.1 Food industry . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 148 I 5.3.2 Applications for biotechnology . .......................... 150 5.4 Conclusions ............... . . . . . . ........ ......... 151 5.5 References . . . . . . . . . . . ....................... 152 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Ion-exchange and electrodialysis.. 155 A. S. Grandison 6.1 Ion-exchange . . . . . . . . . . . . . . . . . . . . ......................... 155 6.1.1 Theory, materials and equipment Solute/ion-exchanger interactions . . . . . , , . . . . . . . . . . . . . . . . . . . . 155 Ion-exchange groups . . . . . . . . . . . . . , , , , . . . . . . . . . . . . . . . . . . . . . 158 Ion-exchange materials . . . . . . . . . . . . . . . . . . . . . . . . . ....................... .................... Elution ................................................. 159 Ion-exchange columns ......................... 160 Mixed bed systems . . . ............................... 160 Stirredtanks ............................................ 160 6.1.2 Applications of ion-exchange in the food and biotechnology industries 160 Softening ............................................... 161 Demineralisation . . . . . . . . . . . . . . . . . . , . . . . . . . . . . . . . . . . . . . . . 16 1 Decolorisation . . . . . ............................ Protein purification . . . ................................ 163 Purification of other compounds . . . . . . . . . . . , . . . . . . . . . 6.2 Electrodialysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ........ 166 6.2.1 Theory and equipment . . . . . . . ...................... 167 6.2.2 Applications of ED in the food an 6.3 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 Innovative separation methods in bioprocessing 179 J. A. Asenjo and J. B. Chaudhuri 7.1 Introduction .................................................... 179 7.2 System characteristics . . . . . . . . . . . . , . . , . . . . . . . , . . . . . . , , . . . . . . . . . . . . 180 7.2.1 Physicochemical basis for separation operations . . . . . . . . . . . . . . . 180 , , , , 7.2.2 Kinetics and mass transfer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18 1 , , , 7.3 Liquid-liquid extraction: introduction , . , , , . . . . . . . . . . . , . . . . . . . . . . . . . . , 181 7.3.1 Aqueous two-phase separation . . . . . . . . . . . . . . . . . . . . . . . . 182 , , , 7.3.2 Reverse micelle extraction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 185 , Contents ix 7.3.3 Perfluorocarbon affinity separations .............. ........... 7.4.1 Adsorption system 7.4.2 Continuous adsorption recycle extraction. ........ 7.4.3 Membrane chromatography ............................. 7.4.4 Chromatographic and adsorption materials ........ 201 7.5 Other developments ......... .......... 7.5.1 Electrically enhanced separations ... .................. 202 ................. 7.6 References ............ ............. 204 .................. .......................... 8 Fractionation of fat , 207 K. K. Rajah 8.1 Introduction .................... ................ .......... ........... 210 8.2 Dry fractionation ................ ................ 211 8.2.1 Flat-bed vac .................... Vacuband batch filter. .................... 8.2.2 Rotary drum filters ................. .............. 215 8.2.3 Membrane filters ...... ............... Low pressure ............. ................... ........ 224 .................... 8.3 Detergent fractionation ................ ................ 232 8.4 Solvent fractionation ...... ............. 8.5 References .................... ................ 238 ....................................... 9 Solids separation processes 243 M. J. Lewis 9.1 Introduction ..... .............. 9.2 Physical properties of solids. ............ ................ 244 9.2.1 Classification of powders ............. 9.2.2 Particle size and particle size distribution ................... 247 9.2.3 Particle density ..................... 9.2.4 Forces of adh ...................... 252 9.2.5 Bulk properties ........... 9.2.6 Bulk density and porosity ............. 9.2.7 Flowability ..... ..................... x Contents 9.3 Separation of particulates and powders ............................... 256 9.3.1 Size reduction .............................................. 256 9.3.2 Sieving ................................................... 258 9.4 Air classification ................................................. 260 9.4.1 Introduction ................................................. 260 9.4.2 Commercial air classifiers .................................... 262 9.4.3 Process characterisation ...................................... 264 9.4.4 Applications ............................................... 268 9.4.5 Cereal separations .......................................... 268 9.4.6 Legumes .................................................. 270 9.4.7 Other applications .......................................... 273 9.5 Wet separation processes .......................................... 273 9.5.1 Protein recovery .......... 9.5.2 Soya processing ......................... 9.5.3 Wheat protein .................................... 9.5.4 Other applications ................ 9.6 Some miscellaneous solids separations ......................... 9.6.1 Dehulling ........................................... 9.6.2 Peeling ................................................... 279 9.6.3 Cleaning of raw materials ..................................... 279 9.6.4 Sorting and grading ......................................... 281 Colour sorting and grading ................................. 281 9.7 References ..................................................... 283 .............................................................. Index 287